CN103965900A - Terbium-doped lead-cadmium fluoride up-conversion luminescent material, its preparation method and organic light-emitting diode - Google Patents
Terbium-doped lead-cadmium fluoride up-conversion luminescent material, its preparation method and organic light-emitting diode Download PDFInfo
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- CN103965900A CN103965900A CN201310037435.9A CN201310037435A CN103965900A CN 103965900 A CN103965900 A CN 103965900A CN 201310037435 A CN201310037435 A CN 201310037435A CN 103965900 A CN103965900 A CN 103965900A
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Abstract
The invention discloses a terbium-doped lead-cadmium fluoride up-conversion luminescent material. The terbium-doped lead-cadmium fluoride up-conversion luminescent material has a general chemical formula of PbyCd1-yF2: xTb<3+>, wherein x is in a range of 0.01-0.08 and y is in a range of 0. 1-0.8. In the photoluminescence spectrum of the terbium-doped lead-cadmium fluoride up-conversion luminescent material, the terbium-doped lead-cadmium fluoride up-conversion luminescent material has excitation wavelength of 796nm, and in the zone of the wavelength of 485nm, 5D4-to-7F6 transition radiation of Tb<3+> ions is produced so that a luminescence peak is formed. The terbium-doped lead-cadmium fluoride up-conversion luminescent material can be used as a blue light emitting material. The invention also provides a preparation method of the terbium-doped lead-cadmium fluoride up-conversion luminescent material and an organic light-emitting diode using the terbium-doped lead-cadmium fluoride up-conversion luminescent material.
Description
Technical field
The present invention relates to a kind of terbium doped plumbous cadmium converting luminescent material of fluoride, preparation method and Organic Light Emitting Diode.
Background technology
Organic Light Emitting Diode (OLED) because unit construction is simple, the characteristic such as cheap, the luminous of production cost, reaction times be short, flexible, apply widely and obtained the utmost point.But owing to obtaining at present, the OLED blue light material of stability and high efficiency is more difficult, has limited greatly the development of white light OLED device and light source industry.
Upconverting fluorescent material can be launched visible ray under long wave (as infrared) radiation excitation, even UV-light, is with a wide range of applications in fields such as optical fiber communication technology, fibre amplifier, 3 D stereo demonstration, biomolecules fluorescence labelling, infrared detectives.But, can be by infrared, the long-wave radiations such as red-green glow inspire the terbium doped plumbous cadmium converting luminescent material of fluoride of blue emission, have not yet to see report.
Summary of the invention
Based on this, being necessary to provide a kind of can be inspired terbium doped plumbous cadmium converting luminescent material of fluoride, the preparation method of blue light and be used the Organic Light Emitting Diode of this terbium doped plumbous cadmium converting luminescent material of fluoride by long-wave radiation.
A kind of terbium doped plumbous cadmium converting luminescent material of fluoride, has following chemical formula Pb
ycd
1-yf
2: xTb
3+, wherein, x is that 0.01～0.08, y is 0.1～0.8.
X is that 0.05, y is 0.6.
A preparation method for terbium doped plumbous cadmium converting luminescent material of fluoride, comprises the following steps:
According to Pb
ycd
1-yf
2: xTb
3+the stoichiometric ratio of each element takes PbF
2, CdF
2and TbF
3powder, wherein, x is that 0.01～0.08, y is 0.1～0.8;
The powder taking is dissolved in to acid solvent, adds afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously;
It is 7～9 that adjusting contains sedimentary mixture pH value, then filters, and with dehydrated alcohol and distilled water wash, is precipitated thing; And
Throw out is dried at 900 DEG C～1400 DEG C to burning, drying the burning time is 2 hours～5 hours, and obtaining chemical general formula is Pb
ycd
1-yf
2: xTb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
Described x is that 0.05, y is 0.6.
Described acid solvent is hydrofluoric acid, Neutral ammonium fluoride or ammonium bifluoride.
Described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
Described basic solvent is ammoniacal liquor.
Described pH value is 8.
Described throw out is transferred in retort furnace and is dried and burn at 1200 DEG C, and drying the burning time is 3 hours.
A kind of Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the encapsulated layer that stack gradually, in described encapsulated layer, doped with terbium doped plumbous cadmium converting luminescent material of fluoride, the chemical general formula of this terbium doped plumbous cadmium converting luminescent material of fluoride is Pb
ycd
1-yf
2: xTb
3+, wherein, x is that 0.01～0.08, y is 0.1～0.8.
The hydrothermal method mild condition of above-mentioned terbium doped plumbous cadmium converting luminescent material of fluoride, synthesis temperature are low more easy to control, and granularity and the pattern of product are controlled, the powder complete crystallization of preparation, good dispersity, cost is lower, produces comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of terbium doped plumbous cadmium converting luminescent material of fluoride of preparation, the excitation wavelength of terbium doped plumbous cadmium converting luminescent material of fluoride is 796nm, in 485nm wavelength zone by Tb
3+ion
5d
4→
7f
6transition radiation form glow peak, can be used as blue light emitting material.
Brief description of the drawings
Fig. 1 is the structural representation of the Organic Light Emitting Diode of an embodiment.
Fig. 2 is the photoluminescence spectrogram of the terbium doped plumbous cadmium converting luminescent material of fluoride prepared of embodiment 1.
Fig. 3 is the XRD spectra of the terbium doped plumbous cadmium converting luminescent material of fluoride prepared of embodiment 1.
Fig. 4 is the spectrogram doped with the Organic Light Emitting Diode of terbium doped plumbous cadmium converting luminescent material of fluoride in the transparent encapsulated layer prepared of embodiment 1.
Embodiment
Below in conjunction with the drawings and specific embodiments, terbium doped plumbous cadmium converting luminescent material of fluoride and preparation method thereof is further illustrated.
The terbium doped plumbous cadmium converting luminescent material of fluoride of one embodiment, has following chemical general formula Pb
ycd
1-yf
2: xTb
3+, wherein, x is that 0.01～0.08, y is 0.1～0.8.
Preferably, x is that 0.05, y is 0.6.
In the photoluminescence spectra of this terbium doped plumbous cadmium converting luminescent material of fluoride, the excitation wavelength of terbium doped plumbous cadmium converting luminescent material of fluoride is 796nm, in the time that material is subject to long wavelength's (as 796nm) radiation, and Tb
3+ion excitation arrives
5d
4excited state, then to the transition of 7F6 energy state, sends the blue light of 485nm, can be used as blue light emitting material.
The preparation method of above-mentioned terbium doped plumbous cadmium converting luminescent material of fluoride, comprises the following steps:
Step S11, according to Pb
ycd
1-yf
2: xTb
3+the stoichiometric ratio of each element takes PbF
2, CdF
2and TbF
3powder, wherein x is that 0.01～0.08, y is 0.1～0.8.
In this step, preferred, x is that 0.05, y is 0.6.
Step S13, will in the powder taking in step S11, add acid solvent, add afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously.
In this step, preferred, described acid solvent is hydrofluoric acid, Neutral ammonium fluoride or ammonium bifluoride.
In this step, preferred, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
In this step, preferred, described basic solvent is ammoniacal liquor.
In this step, dispersion agent is that same ammoniacal liquor splashes into together, and the effect of ammoniacal liquor is neutralization acidity the throw out that produces oxyhydroxide and oxide compound, and dispersion agent effect is that the throw out that prevents generation is reunited.
It is 7～9 that step S15, adjusting contain sedimentary mixture pH value, then filters, and with dehydrated alcohol and distilled water wash, is precipitated thing.
In this step, preferred, described pH value is 8.
Step S17, throw out is dried at 900 DEG C～1300 DEG C to burning, drying the burning time is 2 hours～5 hours, and obtaining chemical general formula is Pb
ycd
1-yf
2: xTb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
In this step, preferred, described throw out is transferred in retort furnace and is dried and burn at 1200 DEG C, and drying the burning time is 3 hours.
The hydrothermal method mild condition of above-mentioned terbium doped plumbous cadmium converting luminescent material of fluoride, synthesis temperature are low more easy to control, and granularity and the pattern of product are controlled, the powder complete crystallization of preparation, good dispersity, cost is lower, produces comparatively environmental protection in simultaneous reactions process without the three wastes; In the photoluminescence spectra of terbium doped plumbous cadmium converting luminescent material of fluoride of preparation, the excitation wavelength of terbium doped plumbous cadmium converting luminescent material of fluoride is 796nm, in 485nm wavelength zone by Tb
3+ion
5d
4→
7f
6transition radiation form glow peak, can be used as blue light emitting material.
Refer to Fig. 1, the Organic Light Emitting Diode 100 of an embodiment, this Organic Light Emitting Diode 100 comprises the substrate 1, negative electrode 2, organic luminous layer 3, transparent anode 4 and the encapsulated layer 5 that stack gradually.In encapsulated layer 5, be dispersed with terbium doped plumbous cadmium converting luminescent material of fluoride 6, the chemical general formula of terbium doped plumbous cadmium converting luminescent material of fluoride is Pb
ycd
1-yf
2: xTb
3+, wherein x is that 0.01～0.08, y is 0.1～0.8.
In the encapsulated layer 5 of Organic Light Emitting Diode 100, be dispersed with terbium doped plumbous cadmium converting luminescent material of fluoride 6, the excitation wavelength of terbium doped plumbous cadmium converting luminescent material of fluoride is 796nm, in 485nm wavelength zone by Tb
3+ion
5d
4→
7f
6transition radiation form glow peak, excite and can launch blue light by red-green glow, blue light mixes the Organic Light Emitting Diode that afterwards formation emits white light with red-green glow.
Be specific embodiment below.
Embodiment 1
Select PbF
2, CdF
2and TbF
3powder is 0.6mmol by each component mole number, 0.4mmol, and 0.05mmol mixes.Mix in rear molten hydrofluoric acid solvent, drip oxalic acid adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 1000 DEG C, obtaining chemical general formula is Pb
0.6cd
0.4f
2: 0.05Tb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
The substrate 1 stacking gradually use soda-lime glass, negative electrode 2 use metal A g layer, organic luminous layer 3 use Ir (piq) 2 (acac) Chinese name two (1-phenyl-isoquinoline 99.9) (methyl ethyl diketones) close iridium (III), transparent anode 4 uses tin indium oxide ITO, and transparent encapsulated layer 5 tetrafluoroethylene.In transparent encapsulated layer 5, be dispersed with terbium doped plumbous cadmium converting luminescent material of fluoride 6, the chemical formula of terbium doped plumbous cadmium converting luminescent material of fluoride is Pb
0.6cd
0.4f
2: 0.05Tb
3+.
Refer to Fig. 2, Figure 2 shows that the terbium doped plumbous cadmium converting luminescent material of fluoride chemical general formula that this enforcement obtains is Pb
0.6cd
0.4f
2: 0.05Tb
3+photoluminescence spectra figure.As seen from Figure 2, the excitation wavelength of the terbium doped plumbous cadmium converting luminescent material of fluoride that the present embodiment obtains is 796nm, in 485nm wavelength zone by Tb
3+ion
5d
4→
7f
6transition radiation form glow peak, this terbium doped plumbous cadmium converting luminescent material of fluoride can be used as blue light emitting material.
Refer to Fig. 3, in Fig. 3, curve is the XRD curve of implementing the terbium doped plumbous cadmium converting luminescent material of fluoride of 1 preparation, test comparison standard P DF card.Contrast PDF card, can find out that diffraction peak is depicted as the crystal orientation of plumbous cadmium fluorochemical, does not occur the relevant peak of praseodymium ytterbium element, illustrates that two kinds of elements are the lattices that entered plumbous cadmium fluorochemical.
Fig. 4 is the spectrogram doped with the Organic Light Emitting Diode of terbium doped plumbous cadmium converting luminescent material of fluoride in the transparent encapsulated layer prepared of embodiment 1, curve 1 is the spectrogram of the terbium doped plumbous cadmium converting luminescent material of fluoride prepared of the embodiment of the present invention, curve 2 is the not contrast doped with terbium doped plumbous cadmium converting luminescent material of fluoride, in figure, can find out, terbium doped plumbous cadmium fluoride glass up-conversion luminescent material can be by the red light of long wave, inspire the blue light of shortwave, after blue light mixes with ruddiness, form white light.
Embodiment 2
Select PbF
2, CdF
2and TbF
3powder is 0.1mmol by each component mole number, 0.9mmol, and 0.08mmol mixes.Mix in rear molten hydrofluoric acid solvent, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 900 DEG C, obtaining chemical general formula is Pb
0.1cd
0.9f
2: 0.08Tb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
Embodiment 3
Select PbF
2, CdF
2and TbF
3powder is 0.8mmol by each component mole number, 0.2mmol, and 0.01mmol mixes.After mixing, be dissolved in hydrofluoric acid solvent, drip trolamine adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 1300 DEG C, obtaining chemical general formula is Pb
0.8cd
0.2f
2: 0.01Tb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
Embodiment 4
Select PbF
2, CdF
2and TbF
3powder is 0.3mmol by each component mole number, 0.7mmol, and 0.02mmol mixes.After mixing, be dissolved in hydrofluoric acid, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2.5 hours at 1100 DEG C, obtaining chemical general formula is Pb
0.3cd
0.7f
2: 0.02Tb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
Embodiment 5
Select PbF
2, CdF
2and TbF
3powder is 0.65mmol by each component mole number, 0.35mmol, and 0.07mmol mixes.After mixing, be dissolved in hydrofluoric acid, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 3 hours at 1000 DEG C, obtaining chemical general formula is Pb
0.65cd
0.35f
2: 0.07Tb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
Embodiment 6
Select PbF
2, CdF
2and TbF
3powder is 0.55mmol by each component mole number, 0.45mmol, and 0.06mmol mixes.After mixing, be dissolved in mass percentage concentration and be in 30% sulfuric acid, drip ethanol adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 4 hours at 950 DEG C, obtaining chemical general formula is Pb
0.55cd
0.45f
2: 0.06Tb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
Embodiment 7
Select PbF
2, CdF
2and TbF
3powder is 0.4mmol by each component mole number, 0.6mmol, and 0.03mmol mixes.After mixing, be dissolved in mass percentage concentration and be in 30% hydrochloric acid solvent, drip oxalic acid adds ammoniacal liquor to make not regeneration precipitation of mixing solutions as dispersion agent simultaneously, continue to drip ammoniacal liquor, regulating the pH value of mixing solutions is 8 left and right, leave standstill and within 2 hours, make precipitation completely, adopt filter cone for filtration collecting precipitation thing, then dehydrated alcohol and distilled water repetitive scrubbing for throw out, finally the throw out of collecting is placed in retort furnace and dried and burn 2 hours at 1000 DEG C, obtaining chemical general formula is Pb
0.4cd
0.6f
2: 0.03Tb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a terbium doped plumbous cadmium converting luminescent material of fluoride, is characterized in that: have following chemical general formula Pb
ycd
1-yf
2: xTb
3+, wherein, x is that 0.01～0.08, y is 0.1～0.8.
2. terbium doped plumbous cadmium converting luminescent material of fluoride according to claim 1, is characterized in that, described x is that 0.05, y is 0.6.
3. a preparation method for terbium doped plumbous cadmium converting luminescent material of fluoride, is characterized in that, comprises the following steps:
According to Pb
ycd
1-yf
2: xTb
3+the stoichiometric ratio of each element takes PbF
2, CdF
2and TbF
3powder, wherein, x is that 0.01～0.08, y is 0.1～0.8;
The powder taking is dissolved in to acid solvent, adds afterwards dispersion agent and basic solvent to obtain containing sedimentary mixture simultaneously;
It is 7～9 that adjusting contains sedimentary mixture pH value, then filters, and with dehydrated alcohol and distilled water wash, is precipitated thing; And
Throw out is dried at 900 DEG C～1400 DEG C to burning, drying the burning time is 2 hours～5 hours, and obtaining chemical general formula is Pb
ycd
1-yf
2: xTb
3+terbium doped plumbous cadmium converting luminescent material of fluoride.
4. the preparation method of terbium doped plumbous cadmium converting luminescent material of fluoride according to claim 3, is characterized in that, described x is that 0.05, y is 0.6.
5. the preparation method of terbium doped plumbous cadmium converting luminescent material of fluoride according to claim 3, is characterized in that, described acid solvent is hydrofluoric acid, Neutral ammonium fluoride or ammonium bifluoride.
6. the preparation method of terbium doped plumbous cadmium converting luminescent material of fluoride according to claim 3, is characterized in that, described dispersion agent is oxalic acid, ethanol, trolamine, water soluble starch or polyoxyethylene glycol.
7. the preparation method of terbium doped plumbous cadmium converting luminescent material of fluoride according to claim 3, is characterized in that, described basic solvent is ammoniacal liquor.
8. the preparation method of terbium doped plumbous cadmium converting luminescent material of fluoride according to claim 3, is characterized in that, described pH value is 8.
9. the preparation method of terbium doped plumbous cadmium converting luminescent material of fluoride according to claim 3, is characterized in that, described throw out is transferred in retort furnace and dried and burn at 1200 DEG C, and drying the burning time is 3 hours.
10. an Organic Light Emitting Diode, comprise the substrate, negative electrode, organic luminous layer, anode and the transparent encapsulated layer that stack gradually, it is characterized in that, in described transparent encapsulated layer, doped with terbium doped plumbous cadmium converting luminescent material of fluoride, the chemical general formula of described terbium doped plumbous cadmium converting luminescent material of fluoride is Pb
ycd
1-yf
2: xTb
3+, wherein, x is that 0.01～0.08, y is 0.1～0.8.
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|---|---|---|---|
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|---|---|---|---|
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Citations (3)
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| CN1842582A (en) * | 2003-08-27 | 2006-10-04 | 皇家飞利浦电子股份有限公司 | Gas discharge lamp with down conversion phosphor |
| KR20110116825A (en) * | 2010-04-20 | 2011-10-26 | 가톨릭대학교 산학협력단 | Light emitting material and organic light emitting diode device including the same |
| CN102787293A (en) * | 2011-05-16 | 2012-11-21 | 海洋王照明科技股份有限公司 | Manganese-doped aluminosilicate oxynitride luminescent film, preparation method and organic electroluminescent devices thereof |
-
2013
- 2013-01-30 CN CN201310037435.9A patent/CN103965900A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1842582A (en) * | 2003-08-27 | 2006-10-04 | 皇家飞利浦电子股份有限公司 | Gas discharge lamp with down conversion phosphor |
| KR20110116825A (en) * | 2010-04-20 | 2011-10-26 | 가톨릭대학교 산학협력단 | Light emitting material and organic light emitting diode device including the same |
| CN102787293A (en) * | 2011-05-16 | 2012-11-21 | 海洋王照明科技股份有限公司 | Manganese-doped aluminosilicate oxynitride luminescent film, preparation method and organic electroluminescent devices thereof |
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